• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The invention relates to a method for the separation of hemicelluloses from biomass digestion process water or spent liquors, with separation of the dissolved solids, concentration of the product and purification of the product by deposition of the inorganic salts and low molecular weight substances. It is characterized in that the conditions of the hemicellulose separation process are set separately at individual separation / purification stages, for example by adjusting the pH. Furthermore, the invention relates to a system for carrying out the process. With such a process and plant it is possible to recover a majority of the dissolved solids - especially xylan and other hemicelluloses.
    公开号:AT519059A1
    申请号:T50780/2016
    申请日:2016-09-02
    公开日:2018-03-15
    发明作者:Oleg Shagaev PhD；Lukas Wiesegger PhD
    申请人:Andritz Ag Maschf；
    IPC主号:
    专利说明:

    Summary
    The invention relates to a process for the separation of hemi-liosis from biomass digestion process water or spent alkalis, with separation of the dissolved solids, concentration of the product and purification of the product by separation of the inorganic salts and substances with a low molecular weight. It is characterized in that the conditions of the hemicellulose separation process are set separately for individual separation / purification stages, for example by setting the pH.
    The invention further relates to a plant for carrying out the process. With such a method and such a system, it is possible to recover a large part of the dissolved solids - in particular xylan and other hemi-liosis.
    2674 ΛΓ / 10
    METHOD FOR SEPARATING SEMI-CELLULOS FROM BIOMASS DIGITAL PROCESS WATER OR USED LYES
    The invention relates to a method for the separation of shark from biomass digestion process water or spent alkalis, with separation of the dissolved solids, concentration of the product and purification of the product by separation of the inorganic salts and substances with a low molecular weight.
    In recent decades, great efforts have been made to develop processes for the separation of valuable organic products from biomass pulping process water (white water from thermomechanical cellulose production (TMP), bleaching presses) - and used alkalis (alkaline pre-hydrolysis, alkaline extraction of kraft pulps for chemical fiber pulps), in particular with regard to the separation of lignin and shark teeth. However, the extracted polymeric semis (e.g. xylo-oligosaccharide (XOS)) are further converted to sugar in a conventional manner, and this in turn either into biofuels (e.g. ethanol) or into other alkaline chemicals such as succinic and lactic acid. The latter are used in the chemical industry for polymer synthesis, for example for polylactic acid (PLA). In the ultrafiltration process, the throughput (river) available to concentrate the wastewater was very low. At the time of reaching this concentration, a throughput of only 10-15 l / m 2 h or less could have a solids content of approx.
    - 3% can be achieved. Such a process could not be used industrially due to the large equipment required for the oil filtration and the still relatively low concentration of the product, in particular for further thermal concentration and / or treatment. This low throughput is mainly due to the contamination of the uitrafiltration units.
    The invention is characterized in that the conditions of the semi-cellulose separation process are set separately for individual separating cleaning steps, for example by adjusting the pH. A high throughput (flow rate) and product concentration can be achieved through these measures.
    An advantageous embodiment of the invention is characterized in that the pH value of the incoming wastewater stream is adjusted to pH 8-11. Such a measure enables a good separation of the fibers, dissolved solids and shark particles.
    A further improvement of the invention is characterized in that the pH of the clear liquid stream is adjusted to pH 8-11, preferably pH 9.0-9.5, after separation of the coarse parts of the dissolved solids. With this setting, the contamination of the filter surfaces, especially the membrane, is significantly reduced.
    A further development of the invention is characterized in that the pH is adjusted to 4.0-4.5 before the inorganic salts are separated off. Such an adjustment of the pH
    2674 AT
    2/10 prevents the binding of sodium ions to the Haibzelluiosen, and these can thus be easily separated.
    An advantageous improvement of the invention is characterized in that the end product enriched with semi-cellulose has a dry content of 15-30% after the ash has been separated off. This enables a more economical subsequent thermal separation treatment.
    Furthermore, the invention relates to a plant for the separation of semi-celluloses from bsomasse process water or spent alkalis, with units for separating the dissolved solids, concentrating the product and purifying the product by separating the inorganic salts and substances with a low molecular weight. This is characterized in that at least one line is provided for adding chemicals to adjust the pH. In this way, high throughputs and concentrations can be achieved.
    An advantageous improvement of the invention is characterized in that a line for adding chemicals is provided in individual separation cleaning units. In this way, the optimal pH value for separation and cleaning can be set.
    An advantageous further development of the invention is characterized in that the units for separating the dissolved solids are designed as mechanical separation devices - such as, for example, centrifuges, filleting or similar devices ---. In this way, the main part of the fibers can be separated and possibly reused in a simple manner.
    A further development of the invention is characterized in that membrane filters are provided as concentration units. These filters are able to separate the fixed solids in high proportions.
    An advantageous improvement of the invention is characterized in that membrane filters are provided as cleaning units, for example for asc. The corresponding product purity can be achieved at the desired level.
    A further improvement of the invention is characterized in that a thermal separation unit is provided for the concentration of the product. de According to requirements, the product can be sold and transported with only a small amount of water.
    The block diagram in FIG. 1 shows the typical structure for the preferred method,
    This process for the separation of shark cell loses can be used in mechanical pulp plants as well as in plants with semi-chemical and chemical digestion processes. It is suitable for installation in existing systems or for conversion projects. The process is for process water from digestion plants for biomass, hardwood (Xyiane) and softwood
    2674 AT 2
    3/10 (Galactoglucomannane, GGM) and in the treatment of spent alkalis, in which an alkaline treatment or water extraction from biomass at high temperature is used.
    Typical digestion plants for separating the semi-cellulose from the process water, bending plants and used alkalis are:
    Hardwood fuel line with aicaline pre-hydrolysis
    Hardwood kraft fabrics with an alkali extraction stage before or after bleaching
    Hardwood NSSC semi-chemical pulp pulping lines Harthoiz green liquor semi-chemical cellulose pulping lines Mechanical and semi-chemical cellulose pulping lines for annual plants (bagasse, kenaf, etc.)
    White water from TMP processes
    APMP Hartholziinien
    BCTMP Harthoizaufschlussverfahren
    The incoming stream A in FIG. 1 can be any wastewater containing semi-cellulose from any mechanical or semi-chemical digestion plant, for example white water or pressate or filtrate or black liquor from cellulose washing machines, normally with a temperature of, for example, 60 ° C. 90 ° C. According to the current state of the art, the incoming stream A, which is burdened with a high chemical oxygen demand (COD), is usually channeled into a wastewater treatment as "wastewater".
    For the process according to the invention, the pH is adjusted to pH 8-11 by stream B. After the first adjustment of the pH value - stream C with coarse dissolved solids, which are not retained during washing, such as fibers and fiber particles and particles larger than> 10 pm - are separated in the first process step I, some separation units also for the separation of particles> 5 pm are designed.
    Process step I can be carried out with mechanical separation equipment such as filtration units or centrifuges (e.g. a decanter centrifuge). For example, the use of a decanter centrifuge is necessary for APMP systems without an existing fiber recovery system (e.g. a disc filter for fiber recovery), with which fiber fragments, fines and other dissolved solids can be separated from the press from screw presses after an alkaline peroxygen process. In this case, the decanter centrifuge is used to remove the dissolved solids. For APMP lines with an existing fiber recovery system (e.g. with a disc filter for fiber recovery), with which fiber fragments, fines and other dissolved solids can be separated from the pressate from cellulose washing devices (e.g. screw presses) after an alkaline peroxide bleaching stage, the use of a decanter centrifuge is optional or can be omitted.
    2674 AT 3
    4.10
    The clear liquid (stream G) in process step I, for example, either with a
    Disc filters or a decanter centrifuge separated coarse parts of the dissolved solids, the wastewater, is stored in a buffer tank; there is adjusted by stream H to pH 8-11 (advantageously to pH 9.0-9.5) to the semi-celluloses with high molecular weight, which at pH <6-r after the re-neutralization stage, which are typical in APMP / BCTMP processes tend to dissolve after the bleaching stage for coagulating and / or absorbing on highly specific surface fine particles / particles. In some applications the pH can only be adjusted by adding the basic chemicals in stream 8, in other applications the addition of chemicals to obtain a pH of 8-11, preferably 9.0-9.5, in stream H done. However, it is also possible to add chemicals in both streams B and H, depending on the properties of the wastewater and the separation units.
    After the high molecular weight semi-celluloses have been desorbed and redissolved, this fraction is introduced into the liquid phase of the wastewater - stream I - and transferred in process step II; Smaller particles in the range> 0 5 --- 10 μm, for example very fine biomass and colloidal dissolved solids (for example silicates, resins), are deposited in this.
    For process step li, machines and equipment such as centrifugal disc separators or other types of separators or microfiltration units with membranes can be used.
    After thorough separation of the dissolved solids and colloidal substances according to process steps I and II, the wastewater J is passed to process step lil, in which the semi-active substances are enriched.
    The reject streams from process step I ~ stream D · and from process specification II - stream E, which contain soft fibers and other dissolved solids with a particle size greater than approx. 0.5 pm, are collected and can be fed into the system (i.e. the mechanical or semi-chemical digestion plant or the pulp and paper mill to be returned - stream F.
    in process step III - uitrafiftration membrane units are usually used, and a large part of the water, the salts and the organic substances with a low molecular weight are separated off and the wastewater / product is concentrated by a factor of 10-20. The permeate from this process step - stream K - which is a significantly lower COD (chemical
    Oxygen requirement) has as stream A, can thus be reused in the system (the mechanical or chemical digestion plant or the pulp and paper mill).
    After process step III, the pH of the concentrated liquor / wastewater L. is adjusted by means of stream M and the resulting stream N is led through the next process step IV - this is carried out with a membrane unit, usually diafiltration, stream N with
    Fresh water or process condensate is washed - stream P - and the inorganic salts (mainly sodium) are separated according to the desired product quality and the product is further concentrated to the content of solids sufficient for the subsequent process step (s). Taking into account that most semi-celluloses
    2674 AT
    5/10 (for example Xyiane) contain uronic acids as beien chains - these are relatively acidic and contain sodium ions bound to COO 'groups - the pH of the stream L is increased with acid, for example with sulfuric acid, hydrochloric acid, etc. - stream M - pH 4.0-4.5 adjusted in order to achieve a more efficient separation of the bound sodium ions (Na + ) and, accordingly, to further reduce the ash content of the product, if necessary,
    Process step SV can deliver the product (stream Q) with a solids concentration of 20-30%. Sn process step SV creates excess water / permeate 0, and this can be used for dilution or any other use in the system, i.e. the mechanical or chemical digestion plant or the pulp and paper mill, instead of fresh water or other process water from the factory. The current Q 'emanating from process step IV is subjected to further treatment in process step V; there the semi-celluloses are further concentrated up to a solids concentration of 50-80%. This process step (V) can usually be a thermal separation, for example an evaporation, in which high-quality excess water, typically condensate, is produced - current R -. This water can be used in the diafilltration stage (step IV), for dilution or for other purposes in the system (the mechanical or chemical digestion plant or the pulp and paper mill) instead of fresh water or other process water from the factory. The thermal drying unit can be heated using steam from the factory. The abehen.de Strem S from process step V can be used as a product, or depending on the requirements regarding the concentration of the end product (for example 80-30% dry substance) in a further process step VI, this can be a drying unit, for example a spray dryer be further thickened. The final product enriched with shark cellulose asked for a dry content of 50-80% as a Schlarom / suspension, paste or gel - stream S - or, if necessary, of about 80-90% as a powder - stream T.
    The invention is not limited to the drawing, but the method can also end after process step IV if the current can continue to be used in the system. Excess water (stream R) from process step V can also be reused instead of fresh water for stream P from process step IV.
    2674 AT
    6.10
    权利要求:
    Claims (10)
    [1]
    Expectations
    1. A process for separating Hemizeliulosen from biomass pulping process water or spent liquors, with deposition of the dissolved solids concentration of the product and purification of the product by precipitation of the inorganic salts and substances having ge r NGEM molecular weight, characterized in that the conditions of hemicellulose deposition process at individual separation cleaning stages can be set separately, for example by adjusting the pH value.
    [2]
    2. The method according to claim 1, characterized in that the pH of the incoming waste water stream (A) is adjusted to pH 8-11.
    [3]
    3. The method according to claim 1 or 2, characterized in that the pH of the clear liquid stream (G) is adjusted to pH 8-11, preferably pH 9.0-9.5 after separation of the coarse parts of the dissolved solids.
    [4]
    4. The method according to any one of claims 1-3, characterized in that the pH is adjusted to 4.0-4.5 before deposition of the inorganic salts.
    [5]
    5. The method according to any one of claims 1-4, characterized in that the end product enriched with hemicellulose has a dry content of 15-30% after separation of the ash.
    [6]
    6. Plant for the separation of hemizeliuloses from biomass digestion process water or spent alkalis, with aggregates for the separation of the dissolved solids, concentration of the product and purification of the product by separation of the inorganic salts and substances with low molecular weight, characterized in that at least one line for addition of chemicals for pH adjustment.
    [7]
    7. Plant according to claim 6, characterized in that a line for the addition of chemicals is provided in each separation / cleaning unit.
    [8]
    8. Plant according to claim 6 or 7, characterized in that the units for separating the dissolved solids as mechanical separation devices - such as centrifuges, filters or similar devices - are designed.
    [9]
    9. Plant according to one of claims 6-8, characterized in that membrane filters are provided as concentration units.
    [10]
    10. Plant according to one of claims 6-9, characterized in that membrane filters are provided as cleaning units, for example for ash separation.
    2574 AT
    7.10
    2574 AT
    8.10
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    引用文献:
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    US20050061457A1|2003-09-23|2005-03-24|Roman Skuratowicz|Process for preparing purified fractions of hemicellulose and cellulose-hemicellulose complexes from alkali treated fiber and products made by the process|
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    CN103541260A|2013-10-28|2014-01-29|宜宾海丝特纤维有限责任公司|Method for recovering hemicellulose from pulping black liquor|
    US4470876A|1982-07-22|1984-09-11|Beaupre Marc F|Kraft overload recovery process|
    FI115978B|2000-11-16|2005-08-31|Ciba Sc Holding Ag|Process for the recovery of non-fibrous substances from wood material|
    AT413697B|2001-11-07|2006-05-15|Andritz Ag Maschf|METHOD FOR TREATING ACIDIC WATER|
    WO2004013409A1|2002-07-25|2004-02-12|Coffin World Water Systems|Apparatus and method for treating black liquor|
    FI120045B|2005-12-22|2009-06-15|Roal Oy|Treatment of cellulose materials and enzymes useful therein|
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    CA2836839A1|2011-05-26|2012-11-29|Liquid Lignin Company, Llc|Process for producing furfural from black liquor|
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    CN104558632B|2014-12-30|2017-01-11|山东龙力生物科技股份有限公司|Method for preparing lignin derivative products from industrial fiber waste residues|
    US11154087B2|2016-02-02|2021-10-26|R.J. Reynolds Tobacco Company|Method for preparing flavorful compounds isolated from black liquor and products incorporating the flavorful compounds|
    CN105714590B|2016-04-15|2017-10-31|广西科学院|Separating lignin and hemicellulose and the method for reclaiming alkali lye from black liquid|
    DE102016219719B3|2016-10-11|2018-01-25|Clariant International Ltd.|Process for recovering cellulose, hemicellulose and lignocellulose from plant biomass|CN111961695A|2020-07-02|2020-11-20|上海昶法新材料有限公司|Method for preparing oligosaccharide by using dissolving pulp precooking waste liquid|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    ATA50780/2016A|AT519059B1|2016-09-02|2016-09-02|Method for separating hemicelluloses from biomass digestion process water or spent alkalis|ATA50780/2016A| AT519059B1|2016-09-02|2016-09-02|Method for separating hemicelluloses from biomass digestion process water or spent alkalis|
    US16/326,769| US10870947B2|2016-09-02|2017-07-27|Process for isolation of hemicelluloses from biomass pulping process waters or spent liquors|
    CA3035614A| CA3035614A1|2016-09-02|2017-07-27|Process for isolation of hemicelluloses from biomass pulping process waters or spent liquors|
    CN201780053705.1A| CN109642394B|2016-09-02|2017-07-27|Method for separating hemicellulose from biomass pulping process water or waste liquid|
    PCT/EP2017/069032| WO2018041488A1|2016-09-02|2017-07-27|Process for isolation of hemicelluloses from biomass pulping process waters or spent liquors|
    JP2019512192A| JP6752359B2|2016-09-02|2017-07-27|Biomass pulping process How to isolate hemicellulose from water or effluent|
    AU2017318207A| AU2017318207B2|2016-09-02|2017-07-27|Process for isolation of hemicelluloses from biomass pulping process waters or spent liquors|
    RU2019106210A| RU2713239C1|2016-09-02|2017-07-27|Method of extracting hemicelluloses from process water from a process of converting biomass to fibrous mass or spent liquors|
    BR112019001781-0A| BR112019001781A2|2016-09-02|2017-07-27|process for isolating hemicelluloses from water from biomass pulp processes or depleted solutions|
    EP17748707.1A| EP3507415B1|2016-09-02|2017-07-27|Process for isolation of hemicelluloses from biomass pulping process waters or spent liquors|
    CL2019000545A| CL2019000545A1|2016-09-02|2019-03-01|Process for the isolation of hemicelluloses from biomass pulp process water or depleted liquors.|
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